CN108192335A - A kind of high intensity polyamide and preparation method thereof - Google Patents
A kind of high intensity polyamide and preparation method thereof Download PDFInfo
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- CN108192335A CN108192335A CN201711472636.6A CN201711472636A CN108192335A CN 108192335 A CN108192335 A CN 108192335A CN 201711472636 A CN201711472636 A CN 201711472636A CN 108192335 A CN108192335 A CN 108192335A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention discloses a kind of high intensity polyamides, belong to resin making technique field, the high intensity polyamide, including following raw material：Polyamide, rosin phenolic resin, ethylene propylene diene rubber, chlorosulfonated polyethylene rubber, fluorubber, hydrogenate nitrile rubber, nitrile rubber, urethane acrylate, alkyd resin, blanc fixe, graphite, zeolite powder, acetylbutyrylcellulose, calcium sulfate crystal whiskers, Triallyl isocyanurate, silicon carbide, active calcium silicate, nano silicon dioxide, nylon, graphite powder, microcrystalline cellulose, silicon powder, white carbon, silane coupling agent KH 560, intensity enhancing auxiliary agent, the high intensity polyamide is by preparing base-material, prepare modified materials, and by base-material, the materials such as modified materials mixing and etc. made of.The polyamide that the present invention is prepared has excellent intensity.
Description
Technical field
The present invention relates to the technical field of resin preparation process more particularly to a kind of high intensity polyamide and its preparations
Method.
Background technology
Polyamide is the condensation polymer type high-molecular compound for having in molecule-CONH structures, it usually by binary acid and
Diamine is obtained through polycondensation.The advantages of polyamide is most prominent is especially narrow for the range of softening point, and not as other thermoplasticity
Resin is such, and there are one the processes for gradually curing or softening, and just cause when temperature is slightly less than fusing point and hastily cure.Polyamide
Resin has preferable resistance to chemical reagents, can resist soda acid and vegetable oil, mineral oil etc..Due in its molecule have amino, carbonyl,
Amide groups isopolarity base, therefore for the modelings such as timber, pottery, paper, cloth, brass, aluminium and phenolic resin, polyester resin, polyethylene
Material all has good glue performance.
A kind of Chinese patent application document " polyamide and preparation method thereof (application publication number：CN105885036A)”
A kind of polyamide and preparation method thereof is disclosed, main chain contains propane diamine unit and oxalic acid unit, wherein, propane diamine list
Member is from the mixture of 1,2- propane diamine, 1,3-PD or both, the preparation method of the polyamide, including as follows
Step：In the presence of the solvent or it is solvent-free in the case of, by diamine monomer system and oxalate diester monomer containing propylene glycol
Mixing in room temperature to prepolymerization is carried out at a temperature of 150 DEG C, obtains prepolymer, and the prepolymer of gained is carried out melt polymerization or solid
Phase-polymerization, obtains polyamide, does not change polyamide high temperature resistant, low water suction, and monomer used is easy to get extensively, price is low
It is honest and clean.But its strength character the needs of can not meeting in actual use.
Invention content
To solve technical problem present in background technology, the present invention proposes a kind of high intensity polyamide and its preparation
Method, to solve in a kind of Chinese patent application document " polyamide and preparation method thereof (application publication number：
CN105885036A the problem of polyamide intensity is insufficient disclosed in) ".
A kind of high intensity polyamide proposed by the present invention, including following raw material：Polyamide, rosin phenolic tree
Fat, ethylene propylene diene rubber, chlorosulfonated polyethylene rubber, fluorubber, hydrogenation nitrile rubber, nitrile rubber, urethane acrylate,
Alkyd resin, blanc fixe, graphite, zeolite powder, acetylbutyrylcellulose, calcium sulfate crystal whiskers, Triallyl isocyanurate, carbon
SiClx, active calcium silicate, nano silicon dioxide, nylon, graphite powder, microcrystalline cellulose, silicon powder, white carbon, silane coupling agent
KH-560, intensity enhancing auxiliary agent；
The silicon powder, white carbon, silane coupling agent KH-560, intensity enhancing auxiliary agent weight ratio be (6-9)：(8-
12)：(2-4)：(18-26).
Further, the silicon powder, white carbon, silane coupling agent KH-560, intensity enhancing auxiliary agent weight ratio be
7.5：10：3：22.
Further, as unit of parts by weight, including following raw material：80-120 parts of polyamide, rosin phenolic resin
20-30 parts, 15-35 parts of ethylene propylene diene rubber, 5-15 parts of chlorosulfonated polyethylene rubber, 4-8 parts of fluorubber, hydrogenation nitrile rubber 3-
9 parts, 2-6 parts of nitrile rubber, 1-5 parts of urethane acrylate, 3-6 parts of alkyd resin, 2-8 parts of blanc fixe, 4-9 parts of graphite,
2-6 parts of zeolite powder, 2-5 parts of acetylbutyrylcellulose, 4-8 parts of calcium sulfate crystal whiskers, 3-6 parts of Triallyl isocyanurate, carbonization
4-8 parts of silicon, 4-9 parts of active calcium silicate, 3-9 parts of nano silicon dioxide, 2-6 parts of nylon, 4-8 parts of graphite powder, microcrystalline cellulose 2-8
Part, 6-9 parts of silicon powder, 8-12 parts of white carbon, 2-4 parts of silane coupling agent KH-560,18-26 parts of intensity enhancing auxiliary agent.
Further, the raw material of the intensity enhancing auxiliary agent includes by weight：15-25 parts of Nano diamond, nano-sized carbon
4-8 parts of SiClx, 3-9 parts of calcium carbonate powder, 10-20 parts of distilled water, 4-8 parts of alkyl phenol polyoxyethylene ether, methyl methacrylate
3-6 parts, 5-15 parts of polypropylene, 4-8 parts of carbamate, 3-9 parts of isopropyl acrylate, 2-8 parts of bromo diethyl malonate, carboxylic
1-5 parts of base NBR latex, 3-6 parts of aluminum sulfate, 2-5 parts of polytetrafluoroethylene (PTFE).
Further, the intensity enhancing auxiliary agent is prepared by following technique：By Nano diamond, nanometer silicon carbide,
Then calcium carbonate powder and distilled water mixed grinding pulp add in alkyl phenol polyoxyethylene ether and methyl methacrylate mixing
Uniformly, 20-40min is ultrasonically treated, then heats to 40-60 DEG C, stirs 20-40min in 800-1200r/min rotating speeds, then
It is cooled to room temperature, in 50-70 DEG C of dry 7-9h, then grinding obtains material a；Then it adds in and polypropylene, ammonia is added in into material a
Carbamate, isopropyl acrylate, bromo diethyl malonate and carboxylic acrylonitrile butadiene rubber latex are uniformly mixed, in 5500-6500r/min
2-4h is stirred under rotating speed, then heats to 90-100 DEG C, keeps the temperature 0.5-1.5h, then adds in aluminum sulfate and polytetrafluoroethylene (PTFE) mixing
Uniformly, it washes, filters, be placed in 45-55 DEG C of baking oven dry 1-4h, be cooled to room temperature to obtain intensity enhancing auxiliary agent.
The present invention also provides a kind of preparation methods of high intensity polyamide, include the following steps：
S1, by polyamide, rosin phenolic resin, ethylene propylene diene rubber, chlorosulfonated polyethylene rubber, fluorubber, hydrogen
Change nitrile rubber, nitrile rubber, urethane acrylate, alkyd resin to be uniformly mixed, 15- is stirred in 650-850/min rotating speeds
25min is warming up to 90-120 DEG C, keeps the temperature 10-20min, then adds in blanc fixe, graphite, zeolite powder, acetate butyrate fiber
Element, calcium sulfate crystal whiskers, Triallyl isocyanurate, silicon carbide, active calcium silicate, nano silicon dioxide, nylon, graphite powder,
Microcrystalline cellulose is uniformly mixed, and ball milling postcooling to room temperature obtains base-material；
S2, silicon powder, white carbon, intensity enhancing auxiliary agent are uniformly mixed, are warming up to 80-90 DEG C, keep the temperature 15-25min, so
Silane coupling agent KH-560 is added in afterwards to be uniformly mixed, and is continuously heating to 110-120 DEG C, is kept the temperature 5-15min, be cooled to room temperature to obtain
Modified materials；
S3, base-material is warming up to 80-90 DEG C, keeps the temperature 15-35min, be subsequently added into modified materials and be uniformly mixed, be cooled to 60-
70 DEG C, 20-30min is kept the temperature, then 1-2h is stirred in 650-850r/min rotating speeds, is cooled to room temperature to obtain high intensity polyamide resin
Fat.
The invention has the advantages that：
(1) by the data of embodiment 1-3 and comparative example 6 as it can be seen that intensity using embodiment 1-3 high intensity polyamides
It significantly improves；Simultaneously by the data of embodiment 1-3 as it can be seen that embodiment 1 is optimum embodiment.
(2) by embodiment 1 and the data of comparative example 1-5 as it can be seen that silicon powder, white carbon, silane coupling agent KH-560, intensity
Reinforcing aids adds play synergistic effect in high intensity polyamide is prepared simultaneously, significantly improves high intensity polyamide
The intensity of resin, this may be：Silicon powder, white carbon, silane coupling agent KH-560, intensity enhancing auxiliary agent are transported as modified system
In the preparation for using polyamide, the graft modification effect of silane coupling agent KH-560 is utilized, realizes silicon powder, hard charcoal
The base-material of black and intensity enhancing auxiliary agent surface hydroxyl and polyamide realizes grafting, imparts excellent strong of polyamide
Degree, while is utilized the wear-resisting humidification of intensity enhancing auxiliary agent, and wherein intensity enhancing auxiliary agent is by by Nano diamond, nanometer
Then silicon carbide, calcium carbonate powder and distilled water mixed grinding pulp add in alkyl phenol polyoxyethylene ether and methacrylic acid
Methyl esters is uniformly mixed, and is ultrasonically treated, is then heated up, and is stirred, is subsequently cooled to room temperature, dry, and then grinding obtains material a；So
After add in polypropylene, carbamate, isopropyl acrylate, bromo diethyl malonate and carboxyl butyronitrile added in into material a
Latex is uniformly mixed, and then stirring heats up, keep the temperature, and then adds in aluminum sulfate and polytetrafluoroethylene (PTFE) is uniformly mixed, and washes, and filters,
Drying in baking oven is placed in, is cooled to room temperature to obtain intensity enhancing auxiliary agent, apply in the preparation of polyamide of the present invention, in silicon
Under the action of alkane coupling agent KH-560, realize and carry out grafting with the major ingredient of polyamide and combined, effectively increase polyamide
The intensity of resin.
Specific embodiment
The present invention is described in detail with reference to specific embodiment, it should be appreciated that embodiment is served only for illustrating this hair
Bright rather than for limiting the invention, any modification made on the basis of the present invention, equivalent replacement etc. are in this hair
In bright protection domain.
In embodiment, the high intensity polyamide, as unit of parts by weight, including following raw material：Polyamide resin
80-120 parts of fat, 20-30 parts of rosin phenolic resin, 15-35 parts of ethylene propylene diene rubber, 5-15 parts of chlorosulfonated polyethylene rubber, fluorine
4-8 parts of rubber, hydrogenation 3-9 parts of nitrile rubber, 2-6 parts of nitrile rubber, 1-5 parts of urethane acrylate, 3-6 parts of alkyd resin,
2-8 parts of blanc fixe, 4-9 parts of graphite, 2-6 parts of zeolite powder, 2-5 parts of acetylbutyrylcellulose, 4-8 parts of calcium sulfate crystal whiskers, triolefin
3-6 parts of propyl isocyanuric acid ester, 4-8 parts of silicon carbide, 4-9 parts of active calcium silicate, 3-9 parts of nano silicon dioxide, 2-6 parts of nylon,
4-8 parts of graphite powder, 2-8 parts of microcrystalline cellulose, 6-9 parts of silicon powder, 8-12 parts of white carbon, 2-4 parts of silane coupling agent KH-560,
18-26 parts of intensity enhancing auxiliary agent.
The intensity enhancing auxiliary agent is prepared by following technique：By weight by 15-25 parts of Nano diamonds, 4-8 parts
Then nanometer silicon carbide, 3-9 part calcium carbonate powder and 10-20 parts of distilled water mixed grinding pulps add in 4-8 parts of alkyl phenols and gather
Ethylene oxide ether and 3-6 parts of methyl methacrylates are uniformly mixed, and are ultrasonically treated 20-40min, are then heated to 40-60 DEG C, in
800-1200r/min rotating speeds stir 20-40min, are subsequently cooled to room temperature, and in 50-70 DEG C of dry 7-9h, then grinding obtains object
Expect a；Then add in into material a add in 5-15 parts of polypropylene, 4-8 parts of carbamates, 3-9 parts of isopropyl acrylates, 2-8 parts
Bromo diethyl malonate and 1-5 parts of carboxylic acrylonitrile butadiene rubber latexes are uniformly mixed, and 2-4h are stirred under 5500-6500r/min rotating speeds, so
After be warming up to 90-100 DEG C, keep the temperature 0.5-1.5h, then add in 3-6 parts of aluminum sulfate and 2-5 parts of polytetrafluoroethylene (PTFE) are uniformly mixed, water
It washes, filters, be placed in 45-55 DEG C of baking oven dry 1-4h, be cooled to room temperature to obtain intensity enhancing auxiliary agent.
The preparation method of the high intensity polyamide, includes the following steps：
S1, by polyamide, rosin phenolic resin, ethylene propylene diene rubber, chlorosulfonated polyethylene rubber, fluorubber, hydrogen
Change nitrile rubber, nitrile rubber, urethane acrylate, alkyd resin to be uniformly mixed, 15- is stirred in 650-850/min rotating speeds
25min is warming up to 90-120 DEG C, keeps the temperature 10-20min, then adds in blanc fixe, graphite, zeolite powder, acetate butyrate fiber
Element, calcium sulfate crystal whiskers, Triallyl isocyanurate, silicon carbide, active calcium silicate, nano silicon dioxide, nylon, graphite powder,
Microcrystalline cellulose is uniformly mixed, and ball milling postcooling to room temperature obtains base-material；
S2, silicon powder, white carbon, intensity enhancing auxiliary agent are uniformly mixed, are warming up to 80-90 DEG C, keep the temperature 15-25min, so
Silane coupling agent KH-560 is added in afterwards to be uniformly mixed, and is continuously heating to 110-120 DEG C, is kept the temperature 5-15min, be cooled to room temperature to obtain
Modified materials；
S3, base-material is warming up to 80-90 DEG C, keeps the temperature 15-35min, be subsequently added into modified materials and be uniformly mixed, be cooled to 60-
70 DEG C, 20-30min is kept the temperature, then 1-2h is stirred in 650-850r/min rotating speeds, is cooled to room temperature to obtain high intensity polyamide resin
Fat.
Below by more specific embodiment, the present invention will be described.
Embodiment 1
A kind of high intensity polyamide, as unit of parts by weight, including following raw material：100 parts of polyamide, rosin
25 parts of phenolic resin, 25 parts of ethylene propylene diene rubber, 10 parts of chlorosulfonated polyethylene rubber, 6 parts of fluorubber, hydrogenation 6 parts of nitrile rubber,
4 parts of nitrile rubber, 3 parts of urethane acrylate, 4.5 parts of alkyd resin, 5 parts of blanc fixe, 6 parts of graphite, 4 parts of zeolite powder, vinegar
Sour 3.5 parts of cellulose butyrate, 6 parts of calcium sulfate crystal whiskers, 4.5 parts of Triallyl isocyanurate, 6 parts of silicon carbide, active calcium silicate 7
Part, 6 parts of nano silicon dioxide, 4 parts of nylon, 6 parts of graphite powder, 5 parts of microcrystalline cellulose, 7.5 parts of silicon powder, 10 parts of white carbon, silicon
3 parts of alkane coupling agent KH-560,22 parts of intensity enhancing auxiliary agent.
The intensity enhancing auxiliary agent is prepared by following technique：By weight by 20 parts of Nano diamonds, 6 parts of nano-sized carbons
Then SiClx, 6 parts of calcium carbonate powders and 15 parts of distilled water mixed grinding pulps add in 6 parts of alkyl phenol polyoxyethylene ether and 4.5
Part methyl methacrylate is uniformly mixed, and is ultrasonically treated 30min, is then heated to 50 DEG C, is stirred in 1000r/min rotating speeds
30min is subsequently cooled to room temperature, and in 60 DEG C of dry 8h, then grinding obtains material a；Then it adds in and 10 parts is added in into material a
Polypropylene, 6 parts of carbamates, 6 parts of isopropyl acrylates, 5 parts of bromo diethyl malonates and 3 parts of carboxylic acrylonitrile butadiene rubber latex mixing
Uniformly, 3h is stirred under 5000r/min rotating speeds, then heats to 95 DEG C, keep the temperature 1h, then add in 4.5 parts of aluminum sulfate and 3.5 parts
Polytetrafluoroethylene (PTFE) is uniformly mixed, and is washed, and is filtered, and is placed in 50 DEG C of baking oven dry 2.5h, is cooled to room temperature to obtain intensity enhancing
Auxiliary agent.
The preparation method of the high intensity polyamide, includes the following steps：
S1, by polyamide, rosin phenolic resin, ethylene propylene diene rubber, chlorosulfonated polyethylene rubber, fluorubber, hydrogen
Change nitrile rubber, nitrile rubber, urethane acrylate, alkyd resin to be uniformly mixed, stir 20min in 750/min rotating speeds, rise
Temperature keeps the temperature 15min to 105 DEG C, then adds in blanc fixe, graphite, zeolite powder, acetylbutyrylcellulose, calcium sulfate crystal whiskers, three
Allyl iso cyanurate, silicon carbide, active calcium silicate, nano silicon dioxide, nylon, graphite powder, microcrystalline cellulose mixing are equal
Even, ball milling postcooling to room temperature obtains base-material；
S2, silicon powder, white carbon, intensity enhancing auxiliary agent are uniformly mixed, are warming up to 85 DEG C, kept the temperature 20min, then add in
Silane coupling agent KH-560 is uniformly mixed, and is continuously heating to 115 DEG C, is kept the temperature 10min, is cooled to room temperature to obtain modified materials；
S3, base-material is warming up to 85 DEG C, keeps the temperature 25min, be subsequently added into modified materials and be uniformly mixed, be cooled to 65 DEG C, heat preservation
25min then stirs 1.5h in 750r/min rotating speeds, is cooled to room temperature to obtain high intensity polyamide.
Embodiment 2
A kind of high intensity polyamide, as unit of parts by weight, including following raw material：80 parts of polyamide, rosin
30 parts of phenolic resin, 15 parts of ethylene propylene diene rubber, 15 parts of chlorosulfonated polyethylene rubber, 4 parts of fluorubber, hydrogenation 9 parts of nitrile rubber,
2 parts of nitrile rubber, 5 parts of urethane acrylate, 3 parts of alkyd resin, 8 parts of blanc fixe, 4 parts of graphite, 6 parts of zeolite powder, acetic acid
2 parts of cellulose butyrate, 3 parts of Triallyl isocyanurate, 8 parts of silicon carbide, 4 parts of active calcium silicate, is received 8 parts of calcium sulfate crystal whiskers
9 parts of silica of rice, 2 parts of nylon, 8 parts of graphite powder, 2 parts of microcrystalline cellulose, 9 parts of silicon powder, 8 parts of white carbon, silane coupling agent
4 parts of KH-560,18 parts of intensity enhancing auxiliary agent.
The intensity enhancing auxiliary agent is prepared by following technique：By weight by 15 parts of Nano diamonds, 8 parts of nano-sized carbons
Then SiClx, 3 parts of calcium carbonate powders and 20 parts of distilled water mixed grinding pulps add in 4 parts of alkyl phenol polyoxyethylene ether and 6 parts
Methyl methacrylate is uniformly mixed, and is ultrasonically treated 20min, is then heated to 60 DEG C, and 40min is stirred in 800r/min rotating speeds,
Room temperature is subsequently cooled to, in 50 DEG C of dry 9h, then grinding obtains material a；Then add in into material a add in 5 parts of polypropylene,
8 parts of carbamates, 3 parts of isopropyl acrylates, 8 parts of bromo diethyl malonates and 1 part of carboxylic acrylonitrile butadiene rubber latex are uniformly mixed, in
2h is stirred under 6500r/min rotating speeds, then heats to 100 DEG C, keeps the temperature 0.5h, then adds in 6 parts of aluminum sulfate and 2 parts of polytetrafluoroethyl-nes
Alkene is uniformly mixed, and is washed, and is filtered, and is placed in 55 DEG C of baking oven dry 1h, is cooled to room temperature to obtain intensity enhancing auxiliary agent.
The preparation method of the high intensity polyamide, includes the following steps：
S1, by polyamide, rosin phenolic resin, ethylene propylene diene rubber, chlorosulfonated polyethylene rubber, fluorubber, hydrogen
Change nitrile rubber, nitrile rubber, urethane acrylate, alkyd resin to be uniformly mixed, stir 25min in 650/min rotating speeds, rise
Temperature keeps the temperature 20min to 90 DEG C, then adds in blanc fixe, graphite, zeolite powder, acetylbutyrylcellulose, calcium sulfate crystal whiskers, three
Allyl iso cyanurate, silicon carbide, active calcium silicate, nano silicon dioxide, nylon, graphite powder, microcrystalline cellulose mixing are equal
Even, ball milling postcooling to room temperature obtains base-material；
S2, silicon powder, white carbon, intensity enhancing auxiliary agent are uniformly mixed, are warming up to 80 DEG C, kept the temperature 25min, then add in
Silane coupling agent KH-560 is uniformly mixed, and is continuously heating to 110 DEG C, is kept the temperature 15min, is cooled to room temperature to obtain modified materials；
S3, base-material is warming up to 80 DEG C, keeps the temperature 35min, be subsequently added into modified materials and be uniformly mixed, be cooled to 60 DEG C, heat preservation
30min then stirs 2h in 650r/min rotating speeds, is cooled to room temperature to obtain high intensity polyamide.
Embodiment 3
A kind of high intensity polyamide, as unit of parts by weight, including following raw material：120 parts of polyamide, rosin
20 parts of phenolic resin, 35 parts of ethylene propylene diene rubber, 5 parts of chlorosulfonated polyethylene rubber, 8 parts of fluorubber, hydrogenation 3 parts of nitrile rubber,
6 parts of nitrile rubber, 1 part of urethane acrylate, 6 parts of alkyd resin, 2 parts of blanc fixe, 9 parts of graphite, 2 parts of zeolite powder, acetic acid
5 parts of cellulose butyrate, 6 parts of Triallyl isocyanurate, 4 parts of silicon carbide, 9 parts of active calcium silicate, is received 4 parts of calcium sulfate crystal whiskers
3 parts of silica of rice, 6 parts of nylon, 4 parts of graphite powder, 8 parts of microcrystalline cellulose, 6 parts of silicon powder, 12 parts of white carbon, silane coupling agent
2 parts of KH-560,26 parts of intensity enhancing auxiliary agent.
The intensity enhancing auxiliary agent is prepared by following technique：By weight by 25 parts of Nano diamonds, 4 parts of nano-sized carbons
Then SiClx, 9 parts of calcium carbonate powders and 10 parts of distilled water mixed grinding pulps add in 8 parts of alkyl phenol polyoxyethylene ether and 3 parts
Methyl methacrylate is uniformly mixed, and is ultrasonically treated 40min, is then heated to 40 DEG C, and 20min is stirred in 1200r/min rotating speeds,
Room temperature is subsequently cooled to, in 70 DEG C of dry 7h, then grinding obtains material a；Then it adds in and 15 parts poly- third is added in into material a
Alkene, 4 parts of carbamates, 9 parts of isopropyl acrylates, 2 parts of bromo diethyl malonates and 5 parts of carboxylic acrylonitrile butadiene rubber latex mixing are equal
It is even, 4h is stirred under 5500r/min rotating speeds, then heats to 90 DEG C, keeps the temperature 1.5h, then adds in 3 parts of aluminum sulfate and 5 parts poly- four
Vinyl fluoride is uniformly mixed, and is washed, and is filtered, and is placed in 45 DEG C of baking oven dry 4h, is cooled to room temperature to obtain intensity enhancing auxiliary agent.
The preparation method of the high intensity polyamide, includes the following steps：
S1, by polyamide, rosin phenolic resin, ethylene propylene diene rubber, chlorosulfonated polyethylene rubber, fluorubber, hydrogen
Change nitrile rubber, nitrile rubber, urethane acrylate, alkyd resin to be uniformly mixed, stir 15min in 850/min rotating speeds, rise
Temperature keeps the temperature 10min to 120 DEG C, then adds in blanc fixe, graphite, zeolite powder, acetylbutyrylcellulose, calcium sulfate crystal whiskers, three
Allyl iso cyanurate, silicon carbide, active calcium silicate, nano silicon dioxide, nylon, graphite powder, microcrystalline cellulose mixing are equal
Even, ball milling postcooling to room temperature obtains base-material；
S2, silicon powder, white carbon, intensity enhancing auxiliary agent are uniformly mixed, are warming up to 90 DEG C, kept the temperature 15min, then add in
Silane coupling agent KH-560 is uniformly mixed, and is continuously heating to 120 DEG C, is kept the temperature 5min, is cooled to room temperature to obtain modified materials；
S3, base-material is warming up to 90 DEG C, keeps the temperature 15min, be subsequently added into modified materials and be uniformly mixed, be cooled to 70 DEG C, heat preservation
20min then stirs 1h in 850r/min rotating speeds, is cooled to room temperature to obtain high intensity polyamide.
Comparative example 1
It is essentially identical with the preparation process of embodiment 1, it has only the difference is that in the raw material of preparation high intensity polyamide
Lack silicon powder, white carbon, silane coupling agent KH-560, intensity enhancing auxiliary agent.
Comparative example 2
It is essentially identical with the preparation process of embodiment 1, it has only the difference is that in the raw material of preparation high intensity polyamide
Lack silicon powder.
Comparative example 3
It is essentially identical with the preparation process of embodiment 1, it has only the difference is that in the raw material of preparation high intensity polyamide
Lack white carbon.
Comparative example 4
It is essentially identical with the preparation process of embodiment 1, it has only the difference is that in the raw material of preparation high intensity polyamide
Lack silane coupling agent KH-560.
Comparative example 5
It is essentially identical with the preparation process of embodiment 1, it has only the difference is that in the raw material of preparation high intensity polyamide
Lack intensity enhancing auxiliary agent.
Comparative example 6
Using a kind of Chinese patent application document " polyamide and preparation method thereof (application publication number：
CN105885036A) " technique of embodiment 1 prepares polyamide.
The polyamide for measuring embodiment 1-3 and comparative example 1-6 carries out indices detection, and obtained testing result is such as
Following table：
| Experimental project | Tensile strength (Mpa) |
| Embodiment 1 | 356.9 |
| Embodiment 2 | 342.7 |
| Embodiment 3 | 348.9 |
| Comparative example 1 | 134.7 |
| Comparative example 2 | 336.4 |
| Comparative example 3 | 334.1 |
| Comparative example 4 | 335.8 |
| Comparative example 5 | 339.4 |
| Comparative example 6 | 106 |
(1) by the data of embodiment 1-3 and comparative example 6 as it can be seen that intensity using embodiment 1-3 high intensity polyamides
It significantly improves；Simultaneously by the data of embodiment 1-3 as it can be seen that embodiment 1 is optimum embodiment.
(2) by embodiment 1 and the data of comparative example 1-5 as it can be seen that silicon powder, white carbon, silane coupling agent KH-560, intensity
Reinforcing aids adds play synergistic effect in high intensity polyamide is prepared simultaneously, significantly improves high intensity polyamide
The intensity of resin, this may be：Silicon powder, white carbon, silane coupling agent KH-560, intensity enhancing auxiliary agent are transported as modified system
In the preparation for using polyamide, the graft modification effect of silane coupling agent KH-560 is utilized, realizes silicon powder, hard charcoal
The base-material of black and intensity enhancing auxiliary agent surface hydroxyl and polyamide realizes grafting, imparts excellent strong of polyamide
Degree, while is utilized the wear-resisting humidification of intensity enhancing auxiliary agent, and wherein intensity enhancing auxiliary agent is by by Nano diamond, nanometer
Then silicon carbide, calcium carbonate powder and distilled water mixed grinding pulp add in alkyl phenol polyoxyethylene ether and methacrylic acid
Methyl esters is uniformly mixed, and is ultrasonically treated, is then heated up, and is stirred, is subsequently cooled to room temperature, dry, and then grinding obtains material a；So
After add in polypropylene, carbamate, isopropyl acrylate, bromo diethyl malonate and carboxyl butyronitrile added in into material a
Latex is uniformly mixed, and then stirring heats up, keep the temperature, and then adds in aluminum sulfate and polytetrafluoroethylene (PTFE) is uniformly mixed, and washes, and filters,
Drying in baking oven is placed in, is cooled to room temperature to obtain intensity enhancing auxiliary agent, apply in the preparation of polyamide of the present invention, in silicon
Under the action of alkane coupling agent KH-560, realize and carry out grafting with the major ingredient of polyamide and combined, effectively increase polyamide
The intensity of resin.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (6)
1. a kind of high intensity polyamide, which is characterized in that including following raw material：Polyamide, rosin phenolic resin, three
First EP rubbers, chlorosulfonated polyethylene rubber, fluorubber, hydrogenation nitrile rubber, nitrile rubber, urethane acrylate, alkyd
Resin, blanc fixe, graphite, zeolite powder, acetylbutyrylcellulose, calcium sulfate crystal whiskers, Triallyl isocyanurate, carbonization
Silicon, active calcium silicate, nano silicon dioxide, nylon, graphite powder, microcrystalline cellulose, silicon powder, white carbon, silane coupling agent KH-
560th, intensity enhancing auxiliary agent；
The silicon powder, white carbon, silane coupling agent KH-560, intensity enhancing auxiliary agent weight ratio be (6-9)：(8-12)：(2-
4)：(18-26).
2. high intensity polyamide according to claim 1, which is characterized in that the silicon powder, white carbon, silane are even
Join agent KH-560, the weight ratio of intensity enhancing auxiliary agent is 7.5：10：3：22.
3. high intensity polyamide according to claim 1 or 2, which is characterized in that as unit of parts by weight, including with
Lower raw material：80-120 parts of polyamide, 20-30 parts of rosin phenolic resin, 15-35 parts of ethylene propylene diene rubber, the poly- second of chlorosulfonation
5-15 parts of alkene rubber, 4-8 parts of fluorubber, hydrogenation 3-9 parts of nitrile rubber, 2-6 parts of nitrile rubber, 1-5 parts of urethane acrylate,
3-6 parts of alkyd resin, 2-8 parts of blanc fixe, 4-9 parts of graphite, 2-6 parts of zeolite powder, 2-5 parts of acetylbutyrylcellulose, calcium sulfate
4-8 parts of whisker, 3-6 parts of Triallyl isocyanurate, 4-8 parts of silicon carbide, 4-9 parts of active calcium silicate, nano silicon dioxide 3-9
Part, 2-6 parts of nylon, 4-8 parts of graphite powder, 2-8 parts of microcrystalline cellulose, 6-9 parts of silicon powder, 8-12 parts of white carbon, silane coupling agent
2-4 parts of KH-560,18-26 parts of intensity enhancing auxiliary agent.
4. according to claim 1-3 any one of them high intensity polyamides, which is characterized in that the intensity enhancing auxiliary agent
Raw material include by weight：15-25 parts of Nano diamond, 4-8 parts of nanometer silicon carbide, 3-9 parts of calcium carbonate powder, distilled water
10-20 parts, 4-8 parts of alkyl phenol polyoxyethylene ether, 3-6 parts of methyl methacrylate, 5-15 parts of polypropylene, carbamate 4-8
Part, 3-9 parts of isopropyl acrylate, 2-8 parts of bromo diethyl malonate, 1-5 parts of carboxylic acrylonitrile butadiene rubber latex, 3-6 parts of aluminum sulfate, poly- four
2-5 parts of vinyl fluoride.
5. according to claim 1-4 any one of them high intensity polyamides, which is characterized in that the intensity enhancing auxiliary agent
It is prepared by following technique：By Nano diamond, nanometer silicon carbide, calcium carbonate powder and distilled water mixed grinding pulp,
Then it adds in alkyl phenol polyoxyethylene ether and methyl methacrylate is uniformly mixed, be ultrasonically treated 20-40min, then heat to
40-60 DEG C, 20-40min is stirred in 800-1200r/min rotating speeds, is subsequently cooled to room temperature, in 50-70 DEG C of dry 7-9h, then
Grinding obtains material a；Then it adds in and polypropylene, carbamate, isopropyl acrylate, bromomalonic acid is added in into material a
Diethylester and carboxylic acrylonitrile butadiene rubber latex are uniformly mixed, and are stirred 2-4h under 5500-6500r/min rotating speeds, are then heated to 90-100
DEG C, 0.5-1.5h is kept the temperature, then aluminum sulfate is added in and polytetrafluoroethylene (PTFE) is uniformly mixed, is washed, is filtered, is placed in 45-55 DEG C of baking
Dry 1-4h, is cooled to room temperature to obtain intensity enhancing auxiliary agent in case.
A kind of 6. preparation method according to claim 1-5 any one of them high intensity polyamides, which is characterized in that packet
Include following steps：
S1, by polyamide, rosin phenolic resin, ethylene propylene diene rubber, chlorosulfonated polyethylene rubber, fluorubber, hydrogenation fourth
Fine rubber, nitrile rubber, urethane acrylate, alkyd resin are uniformly mixed, and 15- is stirred in 650-850/min rotating speeds
25min is warming up to 90-120 DEG C, keeps the temperature 10-20min, then adds in blanc fixe, graphite, zeolite powder, acetate butyrate fiber
Element, calcium sulfate crystal whiskers, Triallyl isocyanurate, silicon carbide, active calcium silicate, nano silicon dioxide, nylon, graphite powder,
Microcrystalline cellulose is uniformly mixed, and ball milling postcooling to room temperature obtains base-material；
S2, silicon powder, white carbon, intensity enhancing auxiliary agent are uniformly mixed, are warming up to 80-90 DEG C, keep the temperature 15-25min, Ran Houjia
Enter silane coupling agent KH-560 to be uniformly mixed, be continuously heating to 110-120 DEG C, keep the temperature 5-15min, be cooled to room temperature and be modified
Material；
S3, base-material is warming up to 80-90 DEG C, keeps the temperature 15-35min, be subsequently added into modified materials and be uniformly mixed, be cooled to 60-70 DEG C,
20-30min is kept the temperature, then 1-2h is stirred in 650-850r/min rotating speeds, is cooled to room temperature to obtain high intensity polyamide.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109096737A (en) * | 2018-07-17 | 2018-12-28 | 全椒祥瑞塑胶有限公司 | A kind of automotive upholstery engineering plastics |
| CN109135263A (en) * | 2018-07-17 | 2019-01-04 | 全椒祥瑞塑胶有限公司 | A kind of preparation method of counter-bending polyamide for automobile interiors |
| CN111040442A (en) * | 2019-12-26 | 2020-04-21 | 富适扣铁路器材(浙江)有限公司 | Whisker-reinforced hydrophobic nylon 66 composite material and preparation method thereof |
| CN111690320A (en) * | 2020-06-24 | 2020-09-22 | 赣县洪顺工艺厂 | High-adhesion toy coating resin and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106700562A (en) * | 2016-12-16 | 2017-05-24 | 安徽亚兰密封件有限公司 | High-hardness wear-resistant rubber sealing piece and preparation method thereof |
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2017
- 2017-12-29 CN CN201711472636.6A patent/CN108192335A/en not_active Withdrawn
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106700562A (en) * | 2016-12-16 | 2017-05-24 | 安徽亚兰密封件有限公司 | High-hardness wear-resistant rubber sealing piece and preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109096737A (en) * | 2018-07-17 | 2018-12-28 | 全椒祥瑞塑胶有限公司 | A kind of automotive upholstery engineering plastics |
| CN109135263A (en) * | 2018-07-17 | 2019-01-04 | 全椒祥瑞塑胶有限公司 | A kind of preparation method of counter-bending polyamide for automobile interiors |
| CN111040442A (en) * | 2019-12-26 | 2020-04-21 | 富适扣铁路器材(浙江)有限公司 | Whisker-reinforced hydrophobic nylon 66 composite material and preparation method thereof |
| CN111040442B (en) * | 2019-12-26 | 2022-06-03 | 富适扣铁路器材(浙江)有限公司 | Whisker-reinforced hydrophobic nylon 66 composite material and preparation method thereof |
| CN111690320A (en) * | 2020-06-24 | 2020-09-22 | 赣县洪顺工艺厂 | High-adhesion toy coating resin and preparation method thereof |
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Application publication date: 20180622 |